WO2013121903A1 - Élément de conversion de longueur d'onde et son procédé de fabrication et dispositif électroluminescent et son procédé de fabrication - Google Patents

Élément de conversion de longueur d'onde et son procédé de fabrication et dispositif électroluminescent et son procédé de fabrication Download PDF

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WO2013121903A1
WO2013121903A1 PCT/JP2013/052433 JP2013052433W WO2013121903A1 WO 2013121903 A1 WO2013121903 A1 WO 2013121903A1 JP 2013052433 W JP2013052433 W JP 2013052433W WO 2013121903 A1 WO2013121903 A1 WO 2013121903A1
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emitting device
wavelength conversion
light emitting
light
manufacturing
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PCT/JP2013/052433
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English (en)
Japanese (ja)
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後藤　賢治
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コニカミノルタ株式会社
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Priority to EP13749248.4A priority Critical patent/EP2816620A4/fr
Priority to US14/377,649 priority patent/US20160013368A1/en
Publication of WO2013121903A1 publication Critical patent/WO2013121903A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/507—Wavelength conversion elements the elements being in intimate contact with parts other than the semiconductor body or integrated with parts other than the semiconductor body
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/52—Encapsulations
    • H01L33/56—Materials, e.g. epoxy or silicone resin
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/293—Organic, e.g. plastic
    • H01L23/296—Organo-silicon compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/11—Device type
    • H01L2924/12—Passive devices, e.g. 2 terminal devices
    • H01L2924/1204—Optical Diode
    • H01L2924/12041—LED
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/11—Device type
    • H01L2924/12—Passive devices, e.g. 2 terminal devices
    • H01L2924/1204—Optical Diode
    • H01L2924/12042—LASER
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
    • H01L2924/181—Encapsulation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/005—Processes relating to semiconductor body packages relating to encapsulations

Definitions

  • the present invention relates to a light emitting device having a light emitting element and a wavelength conversion unit that converts the wavelength of light emitted from the light emitting element.
  • phosphors such as YAG (yttrium, aluminum, garnet) phosphors are arranged in the vicinity of gallium nitride (GaN) blue LED (Light Emitting Diode) chips, and blue light emitted from the blue LED chips.
  • GaN gallium nitride
  • a technique for obtaining a white light emitting device by color mixture of yellow light emitted when the phosphor receives blue light and emits secondary light is widely used.
  • a technique for obtaining a white light emitting device by mixing blue light emitted from a blue LED chip and red light and green light emitted by each phosphor receiving blue light and secondary light emission is also used. Yes.
  • Such white light emitting devices have various uses, for example, there is a demand as an alternative to fluorescent lamps and incandescent lamps. In addition, it is also being used for lighting devices such as automobile headlights that require extremely high luminance. Since the headlight is required to have high visibility with respect to an object such as a distant sign, high performance is also required in terms of the color of the white light emitting device and the color uniformity of the irradiation range.
  • a method of sealing an LED chip or a mounting portion using a transparent resin in which a phosphor is dispersed is generally used.
  • the specific gravity of the phosphor particles is larger than that of the transparent resin.
  • the phosphor settles before the transparent resin is cured, and color unevenness occurs during light emission.
  • the luminous efficiency is lowered due to the sulfuration and discoloration of the metal electrode and the metal reflection part.
  • Patent Document 1 discloses a light-emitting device that attempts to suppress sedimentation and segregation of a phosphor by using a silicone resin having a viscosity of 100 to 10,000 mPa ⁇ s when cured as a sealing body.
  • Patent Document 2 discloses a light-emitting device in which a liquid translucent sealing material is added with a lipophilic compound obtained by adding an organic cation to a layered compound mainly composed of a viscous mineral as an anti-settling material for a phosphor, and the light emitting device A manufacturing method is disclosed.
  • Patent Document 3 discloses a configuration in which a barrier layer for preventing sulfidation is provided.
  • Patent Documents 1 and 2 the problem of uneven color due to sedimentation of the phosphor is improved to some extent.
  • phosphors are dispersed in a resin in any document, when used in a high-luminance lighting device as described above, the heat generated by the LED itself or the heat generated by the phosphor excited by the LED light is used. As a result, the resin is deteriorated and colored, whereby the transmittance may be reduced, and problems such as uneven color and surface scattering due to deformation of the resin may occur.
  • the technique of Patent Document 3 is not sufficient as a measure for preventing sulfidation.
  • An object of the present invention is to reduce the occurrence of color unevenness to the extent that it can be sufficiently used in applications where color uniformity is required, such as lighting, and to improve the antisulfurization performance and light extraction efficiency. It is an object of the present invention to provide a manufacturing method, a wavelength conversion element thereof, a manufacturing method of a light emitting device, and the light emitting device.
  • the present invention provides a step of applying a first liquid mixture containing a phosphor, swellable particles, inorganic particles, and a first solvent on a light emitting element, and a translucent ceramic material on the step. And a step of applying and heating the second mixed liquid containing the second solvent, and further applying a step of applying and heating the silicone sealing agent thereon.
  • the second mixed liquid contains water and / or inorganic particles.
  • the inorganic particles are preferably a metal oxide.
  • the silicone sealant is preferably phenyl silicone.
  • the light-emitting device of the present invention is manufactured by any one of the above-described methods for manufacturing a light-emitting device.
  • the present invention also includes a step of applying a first liquid mixture containing a phosphor, swellable particles, inorganic particles, and a first solvent to at least one surface of a translucent substrate, and a translucent ceramic material and It is set as the manufacturing method of the wavelength conversion element which has the process of apply
  • the second mixed liquid contains water and / or inorganic particles.
  • the inorganic particles are preferably a metal oxide.
  • the silicone sealing agent is preferably phenyl silicone.
  • the wavelength conversion element of the present invention is manufactured by the above-described method for manufacturing a wavelength conversion element.
  • the method for manufacturing a light emitting device of the present invention is obtained by adding a step of installing the wavelength converting element on the light emitting surface side of the light emitting element in the above method for manufacturing a wavelength converting element.
  • the light-emitting device of the present invention is manufactured by the above-described light-emitting device manufacturing method.
  • the present invention it is possible to reduce the occurrence of color unevenness to the extent that it can be sufficiently used in applications where color uniformity is required, such as lighting, and to improve the antisulfurization performance and light extraction efficiency.
  • FIG. 1 is a schematic cross-sectional view of a light emitting device according to a first embodiment of the present invention.
  • a metal part 2 is provided at the bottom of an LED substrate 1 having a concave cross section, and an LED element 3 is disposed on the metal part 2 as a light emitting element.
  • the LED element 3 is provided with a protruding electrode 4 on a surface facing the metal part 2, and the metal part 2 and the LED element 3 are connected via the protruding electrode 4 (flip chip type).
  • a blue LED element is used as the LED element 3.
  • a blue LED element is formed by laminating an n-GaN-based cladding layer, an InGaN light-emitting layer, a p-GaN-based cladding layer, and a transparent electrode on a sapphire substrate.
  • the wavelength conversion part 6 is provided in the recessed part of the LED board 1 so that the LED element 3 may be covered.
  • the wavelength conversion unit 6 includes a wavelength conversion layer 7 that covers the LED element 3, a ceramic layer 8 formed on the wavelength conversion layer 7, and a silicone sealing layer 11 formed on the ceramic layer 8. .
  • the wavelength conversion layer 7 is a part that converts light having a predetermined wavelength emitted from the LED element 3 into light having a different wavelength, and is excited by the wavelength from the LED element 3 to emit fluorescence having a wavelength different from the excitation wavelength. Contains the body.
  • the ceramic layer 8 is a layer for sealing and protecting the wavelength conversion layer 7, and has translucency that transmits at least the light of the LED element 3 and the fluorescence of the wavelength conversion layer 7.
  • the silicone sealing layer 11 is a layer intended to improve gas barrier properties, physical strength, light extraction efficiency, and the like, and has a light-transmitting property that transmits at least the light of the LED element 3 and the fluorescence of the wavelength conversion layer 7. .
  • the configuration and formation method of the wavelength conversion unit 6 (the wavelength conversion layer 7, the ceramic layer 8, and the silicone sealing layer 11) and the method for manufacturing the light emitting device 100 will be described in detail.
  • the wavelength conversion layer 7 is obtained by applying a mixed liquid (first mixed liquid) containing at least a phosphor, swellable particles, inorganic particles (inorganic fine particles), and a solvent (first solvent) and heating (drying). Is a layer.
  • first mixed liquid contains a light-transmitting ceramic material as a binder
  • the chemical reaction occurs over time from the preparation and the viscosity increases, and after 168 hours from the preparation, the viscosity becomes unfavorable for application.
  • the first mixed liquid preferably has a small amount of the binder component, and more preferably does not contain the binder component.
  • the ceramic layer 8 is a transparent ceramic layer (glass body) obtained by applying a mixed liquid (second mixed liquid) containing at least a translucent ceramic material and a solvent (second solvent) and heating (firing). .
  • the second liquid mixture may contain swellable particles, water, inorganic particles, and the like.
  • the silicone sealing layer 11 is a layer obtained by applying a silicone sealing agent containing a silicone resin and heating (curing) it. (Phosphor)
  • the phosphor is excited by the wavelength of the light emitted from the LED element 3 (excitation wavelength) and emits fluorescence having a wavelength different from the excitation wavelength.
  • a YAG (yttrium, aluminum, garnet) phosphor that converts blue light (wavelength 420 nm to 485 nm) emitted from the blue LED element into yellow light (wavelength 550 nm to 650 nm) is used.
  • Such phosphors use oxides of Y, Gd, Ce, Sm, Al, La, and Ga, or compounds that easily become oxides at high temperatures, and are mixed well in a stoichiometric ratio.
  • a mixed raw material is obtained.
  • a coprecipitated oxide obtained by calcining a solution obtained by coprecipitation of a solution obtained by dissolving a rare earth element of Y, Gd, Ce, or Sm in an acid with a stoichiometric ratio with oxalic acid, and aluminum oxide or gallium oxide.
  • an appropriate amount of fluoride such as ammonium fluoride is mixed with the obtained mixed raw material as a flux and pressed to obtain a molded body.
  • the obtained molded body is packed in a crucible and fired in air at a temperature range of 1350 to 1450 ° C. for 2 to 5 hours to obtain a sintered body having the phosphor emission characteristics.
  • the YAG phosphor is used.
  • the type of the phosphor is not limited to this, and other phosphors such as a non-garnet phosphor containing no Ce are used. You can also.
  • the larger the particle size of the phosphor the higher the light emission efficiency (wavelength conversion efficiency), but the gap formed at the interface with the swellable particles becomes larger, and the film strength of the formed wavelength conversion layer 7 decreases. Therefore, in consideration of the size of the gap generated at the interface between the luminous efficiency and the swellable particles, it is preferable to use one having a volume average particle size of 1 ⁇ m to 50 ⁇ m.
  • the volume average particle diameter of the phosphor can be measured by, for example, a Coulter counter method or a laser diffraction / scattering particle diameter measuring apparatus. (Swellable particles)
  • swellable particles fluoride particles such as magnesium fluoride, aluminum fluoride, and calcium fluoride, layered silicate minerals, imogolite, and allophane can be used.
  • layered silicate mineral a swellable clay mineral having a structure such as a mica structure, a kaolinite structure, or a smectite structure is preferable, and a smectite structure rich in swelling properties is more preferable. Since the layered silicate mineral has a card house structure in the mixed solution, it has an effect of greatly increasing the viscosity of the mixed solution in a small amount. Further, since the layered silicate mineral has a flat plate shape, there is an effect of improving the film strength of the wavelength conversion layer 7.
  • the mineral is a solid substance having a certain chemical composition and crystal structure, which is a natural or synthetic inorganic substance.
  • layered silicate minerals include natural or synthetic hectrite, saponite, stevensite, hydelite, montmorillonite, nontrinite, bentonite, and other smectite clay minerals; Examples thereof include swellable mica genus clay minerals such as silicic fluorine mica, Na-type fluorine teniolite, Li-type fluorine teniolite, vermiculite and kaolinite, and mixtures thereof.
  • the content of the swellable particles in the first mixed solution is less than 0.1% by weight, the ratio of solid components such as phosphors, fine particles, and metal alkoxide in the first mixed solution increases, and the dispersibility thereof. Gets worse.
  • the content of the swellable particles exceeds 60% by weight, the scattering of excitation light by the swellable particles is often generated, the emission luminance of the wavelength conversion layer 7 is lowered, and the translucency of the ceramic layer 8 is lowered. Therefore, the content of the swellable particles in the first mixed solution is preferably 0.1% by weight to 60% by weight, and more preferably 0.5% by weight to 30% by weight.
  • the swelling particles have a thickening effect, but if the ratio in the wavelength conversion layer 7 or the ceramic layer 8 is high, the viscosity of the liquid mixture does not increase.
  • the viscosity of the liquid mixture is not limited to other solvents, phosphors, etc. Determined by the ratio with the ingredients.
  • the surface of the swellable particles modified with an ammonium salt or the like can be used as appropriate. (solvent)
  • water As the solvent, water, an organic solvent, or a mixed solvent of water and an organic solvent can be used.
  • Water has a role of swelling hydrophilic swellable particles.
  • the addition of water to the fluoride particles increases the viscosity of the liquid mixture, so that sedimentation of the phosphor can be suppressed.
  • swelling since there exists a possibility that swelling may be inhibited when the impurity is contained in water, it is necessary to use the pure water which does not contain an impurity as the water to add.
  • the organic solvent is used for improving the wettability of the mixed solution and adjusting the viscosity.
  • the addition of an organic solvent to the fluoride particles increases the viscosity of the liquid mixture, so that sedimentation of the phosphor can be suppressed.
  • water is added to the hydrophilic swellable particles to swell, it is preferable to use alcohols such as methanol, ethanol, propanol, and butanol having excellent compatibility with water as the organic solvent. Two or more kinds of alcohols may be combined.
  • the inorganic particles have a filling effect that fills gaps formed at the interface between the phosphor and the swellable particles, and a thickening effect that increases the viscosity of the mixed solution before heating.
  • the inorganic particles used in the present invention include metal oxide fine particles such as silicon oxide, titanium oxide, zinc oxide, aluminum oxide, and zirconium oxide. In consideration of compatibility with ceramic materials and solvents, inorganic particles whose surfaces are treated with a silane coupling agent or a titanium coupling agent can be used as appropriate.
  • the content of the inorganic particles in the wavelength conversion layer 7 is less than 0.5% by weight, the ratio of solid components such as phosphors in the first mixed solution increases, and the dispersibility thereof deteriorates to reduce the content during coating. Handling becomes difficult, and it becomes difficult to apply with uniform chromaticity.
  • the content of the inorganic particles exceeds 70% by weight, the scattering of excitation light by the inorganic particles occurs frequently, and the light emission luminance of the wavelength conversion layer 7 decreases. Therefore, the content of the inorganic particles in the first mixed solution is preferably 0.5% by weight to 70% by weight, more preferably 0.5% by weight to 65% by weight, and more preferably 1% by weight to 60% by weight. The following is more preferable.
  • the inorganic particles have a thickening effect, but if the ratio in the wavelength conversion layer 7 is high, the viscosity of the liquid mixture does not increase.
  • the viscosity of the liquid mixture is a ratio with other components such as a solvent and a phosphor. Determined.
  • the particle size distribution of the inorganic particles is not particularly limited, and may be distributed over a wide range or may be distributed over a relatively narrow range.
  • the central particle diameter of the primary particle diameter is 0.001 ⁇ m or more and 50 ⁇ m or less and is preferably smaller than the phosphor.
  • the average particle diameter of the inorganic particles can be measured, for example, by a Coulter counter method. (Translucent ceramic material)
  • the translucent ceramic material is a ceramic precursor, and an inorganic or organic metal compound can be used.
  • the metal compound include metal alkoxides, metal acetylacetonates, metal carboxylates, metal nitrates, metal oxides, and the like, and metal alkoxides that are easily gelled by hydrolysis and polymerization reaction are preferable.
  • the metal alkoxide may be a single molecule such as tetraethoxysilane, or may be a polysiloxane in which an organic siloxane compound is linked in a chain or a ring, but a polysiloxane that increases the viscosity of the mixed solution is preferable.
  • a translucent glass body can be formed, but it is preferable to contain a silicon
  • the silicone sealant a resin having a structure in which silicon atoms having an organic group such as an alkyl group or an aryl group are alternately bonded to oxygen atoms as a skeleton can be used.
  • the silicone sealing layer 11 can be formed by applying phenyl silicone as a silicone sealing agent on the ceramic layer 8 and heating at 150 ° C. for 1 hour. (Procedure for adjusting the first mixture)
  • a phosphor, swellable particles, inorganic particles (inorganic fine particles), and a solvent (first solvent) may be simply mixed.
  • the preferred viscosity of the first mixed liquid is 10 to 1000 mPa ⁇ s, more preferred viscosity is 12 to 800 mPa ⁇ s, and most preferred viscosity is 20 to 600 mPa ⁇ s.
  • swellable particles, water, and inorganic particles may be mixed in a solution in which a translucent ceramic material is dispersed in a solvent (second solvent) as necessary.
  • a solvent second solvent
  • the sol precursor solution may be heated to be in a gel state and further fired to form a transparent ceramic layer by a so-called sol-gel method.
  • the transparent ceramic layer may be formed directly without forming.
  • a metal alkoxide for example, a metal alkoxide, water for hydrolysis, a solvent, a catalyst, and the like.
  • the catalyst hydrochloric acid, sulfuric acid, nitric acid, acetic acid, hydrofluoric acid, ammonia and the like can be used.
  • the heating temperature of the gel is preferably 120 to 250 ° C., and preferably 120 to 200 ° C. from the viewpoint of further suppressing the deterioration of the LED element 3.
  • the heating temperature after coating is preferably 120 to 500 ° C., and from the viewpoint of further suppressing the deterioration of the LED element 3, 120 to 350 ° C. is preferable.
  • the coating device 10 mainly includes a movable table 20 that can move up and down, left and right, and back and forth, and a spray device 30 that can spray the first mixed liquid.
  • the spray device 30 is disposed above the movable table 20.
  • the spray device 30 has a nozzle 32 into which air is sent, and an air compressor (not shown) for sending air is connected to the nozzle 32.
  • the hole diameter at the tip of the nozzle 32 is 20 ⁇ m to 2 mm, preferably 0.1 to 0.3 mm.
  • the nozzle 32 can move up and down, left and right, and back and forth, like the moving table 20.
  • the spray gun W-101-142BPG manufactured by Anest Iwata is used as the nozzle 32, and the OFP-071C manufactured by Anest Iwata is used as the compressor.
  • the angle of the nozzle 32 can be adjusted, and the nozzle 32 can be tilted with respect to the movable table 20 (or the LED substrate 1 installed on the moving table 20).
  • the angle of the nozzle 32 with respect to the injection target (LED substrate 1) is preferably in the range of 0 to 60 ° when the vertical direction from the injection target is 0 °.
  • a tank 36 is connected to the nozzle 32 via a connecting pipe 34.
  • a first mixed solution 40 is stored in the tank 36.
  • the tank 36 contains a stirring bar, and the first mixed solution 40 is constantly stirred. If the 1st liquid mixture 40 is stirred, sedimentation of the fluorescent substance with large specific gravity can be suppressed, and the state which the fluorescent substance dispersed in the 1st liquid mixture 40 can be hold
  • Anest Iwata PC-51 is used as the tank.
  • a plurality of LED substrates 1 (on which the LED elements 3 are mounted in advance) are installed on the moving table 20, and the positional relationship between the LED substrate 1 and the nozzle 32 of the spray device 30. Is adjusted (position adjustment step).
  • the LED substrate 1 is installed on the moving table 20, and the LED substrate 1 and the tip of the nozzle 32 are arranged to face each other.
  • the first mixed solution 40 can be uniformly applied as the distance between the LED substrate 1 and the nozzle 32 increases, but the film strength also tends to decrease. It is suitable to keep the distance in the range of 3 to 30 cm.
  • the first mixed solution 40 is sprayed from the nozzle 32 and the first mixed solution 40 is applied to the LED substrate 1 while the LED substrate 1 and the nozzle 32 are moved relative to each other (spraying / coating step).
  • the moving base 20 and the nozzle 32 are moved to move the LED substrate 1 and the nozzle 32 back and forth and right and left.
  • Either one of the moving table 20 and the nozzle 32 may be fixed, and the other may be moved back and forth and left and right.
  • a method of applying a plurality of LED elements 3 in a direction orthogonal to the moving direction of the moving table 20 and moving the nozzle 32 in a direction orthogonal to the moving direction of the moving table 20 is also preferably used.
  • the first mixed solution 40 is sprayed from the tip of the nozzle 32 toward the LED substrate 1.
  • the distance between the LED substrate 1 and the nozzle 32 can be adjusted in the above range in consideration of the pressure of the air compressor.
  • the pressure of the compressor is adjusted so that the pressure (spray pressure) at the inlet (tip) of the nozzle 32 is 0.14 MPa.
  • the first mixed liquid 40 can be applied onto the LED element 3.
  • a nozzle that can control the dropping amount of the coating liquid and that does not cause nozzle clogging such as a phosphor is used.
  • a non-contact jet dispenser manufactured by Musashi Engineering Co., Ltd. or its dispenser can be used.
  • an ink jet apparatus a nozzle that can control the discharge amount of the coating liquid and does not cause clogging of nozzles such as phosphors is used.
  • an ink jet apparatus manufactured by Konica Minolta IJ can be used.
  • the wavelength conversion layer 7 having a uniform thickness (uniform phosphor distribution) is formed on the LED element 3 by heating (drying) the first mixed solution thus applied.
  • a predetermined amount of the second mixed liquid is sprayed on the wavelength conversion layer 7 by a spray coating method.
  • the coating apparatus 10 can also be used here. Part of the applied second mixed solution penetrates into the gaps between the phosphor particles and the swellable particles.
  • the ceramic layer 8 is formed by heating (baking) this.
  • the ceramic acts as a binder for the phosphor particles, the swellable particles, and the LED element 3.
  • the ceramic layer 8 is clearly formed on the wavelength conversion layer 7 and has a function of sealing the wavelength conversion layer 7.
  • the thickness of the wavelength conversion layer 7 is preferably 5 ⁇ m or more and 500 ⁇ m or less.
  • a predetermined amount of silicone sealant is applied onto the ceramic layer 8 by a dispenser.
  • the silicone sealing layer 11 is formed by heating (curing) this.
  • FIG. 3 is a schematic sectional view of a light emitting device according to a second embodiment of the present invention.
  • a metal part 2 is provided on a flat LED substrate 1, and the LED element 3 is disposed on the metal part 2 as a light emitting element.
  • the LED element 3 is provided with a protruding electrode 4 on a surface facing the metal part 2, and the metal part 2 and the LED element 3 are connected via the protruding electrode 4 (flip chip type).
  • the wavelength conversion element 9 includes a glass substrate 5 and a wavelength conversion unit 6 formed on the upper surface of the glass substrate 5.
  • the shape of the glass substrate 5 is not particularly limited, and a flat plate shape, a lens shape, or the like can be adopted.
  • the wavelength conversion unit 6 may be formed on the lower surface of the glass substrate 5.
  • the wavelength conversion unit 6 includes a wavelength conversion layer 7 formed on the glass substrate 5, a ceramic layer 8 formed on the wavelength conversion layer 7, and a silicone sealing layer 11 formed on the ceramic layer 8. is doing.
  • a predetermined amount of the first mixed liquid is applied to one side of the glass substrate 5, and heated to form the wavelength conversion layer 7 having a predetermined thickness.
  • a predetermined amount of the second liquid mixture is applied to the upper surface of the wavelength conversion layer 7. Part of the applied second mixed solution penetrates into the gaps between the phosphor particles and the swellable particles.
  • the ceramic layer 8 is formed by baking the glass substrate 5 with which the 2nd liquid mixture was apply
  • a predetermined amount of silicone sealant is applied to the upper surface of the ceramic layer 8.
  • the silicone sealing layer 11 is formed by heating the glass substrate 5 to which the silicone sealing agent is applied.
  • the application method of the first and second mixed liquids and the silicone sealant is not particularly limited, and various conventionally known methods such as a bar coating method, a spin coating method, and a spray coating method can be used. .
  • the light-emitting device 100 can be manufactured by cut
  • size for example, 2x2 mm
  • the glass substrate 5 is used in the said embodiment, if it is a board
  • FIG. 4 is a schematic cross-sectional view of a light emitting device according to a third embodiment of the present invention.
  • the metal part 2 is provided at the bottom of the LED substrate 1 having a concave cross section
  • the LED element 3 is disposed on the metal part 2
  • a lid is provided on the concave part of the LED substrate 1.
  • a wavelength conversion element 9 is provided. Since the configuration of other parts including the wavelength conversion element 9 is the same as that of the second embodiment, the description thereof is omitted.
  • the LED element 3 is disposed in the concave portion of the LED substrate 1, and the wavelength conversion element 9 used in the second embodiment is bonded to the upper end of the side wall of the LED substrate 1 so as to cover the concave portion. Can be manufactured.
  • light emitted from the side surface of the LED element 3 is also efficiently converted into fluorescence as compared with the second embodiment.
  • the shape and size of the concave portion of the LED substrate 1 can be appropriately designed according to the specifications of the light emitting device 102.
  • the side surface of the recess may be tapered.
  • a configuration in which the light emission efficiency of the light emitting device 102 is increased by using the inner surface of the recess as a reflection surface may be employed.
  • the present invention is not limited to the above-described embodiments, and various modifications are possible within the scope shown in the claims, and can be obtained by appropriately combining technical means disclosed in different embodiments. Embodiments are also included in the technical scope of the present invention.
  • a light emitting device that emits white light by using a blue LED and a phosphor together has been described as an example.
  • a green LED or a red LED and a phosphor are used in combination.
  • Examples 1 to 6 are examples of the light emitting device 100 of the first embodiment
  • Comparative Examples 1 and 2 are examples of the light emitting device having the same shape as the light emitting device 100 of the first embodiment.
  • examples of the second and third embodiments are omitted, results similar to those of Examples 1 to 6 were obtained.
  • the phosphor used in each example and comparative example is a mixture of 7.41 g of Y 2 O 3 , 4.01 g of Gd 2 O 3 , 0.63 g of CeO 2 , and 7.77 g of Al 2 O 3 as phosphor raw materials. Then, an aluminum crucible mixed with an appropriate amount of ammonium fluoride as a flux is filled in an aluminum crucible and baked at a temperature range of 1350 to 1450 ° C. for 2 to 5 hours in a reducing atmosphere in which hydrogen-containing nitrogen gas is circulated. Thus, a fired product ((Y 0.72 Gd 0.24 ) 3 Al 5 O 12 : Ce 0.04 ) was obtained.
  • the obtained fired product was pulverized, washed, separated, and dried to obtain yellow phosphor particles having a volume average particle diameter of about 1 ⁇ m.
  • the emission wavelength of excitation light with a wavelength of 465 nm was measured, it had a peak wavelength at a wavelength of approximately 570 nm.
  • the number of g is the mass ratio of each component in the liquid and is different from the amount actually prepared.
  • a first mixed solution was prepared by mixing 0.05 g of a silicic acid-treated silicic acid (manufactured by Nippon Aerosil Co., Ltd.) and 1.5 g of propylene glycol as a solvent.
  • This first mixed solution is sprayed onto the concave portion of the LED substrate 1 and the surface of the LED element 3 at a spray pressure of 0.2 MPa and a moving speed of 100 mm / s using the coating apparatus 10 and heated at 50 ° C. for 1 hour.
  • the wavelength conversion layer 7 was produced by drying.
  • 1 g of a polysiloxane dispersion polysiloxane 14 wt%, isopropyl alcohol 86 wt%) and isopropyl alcohol 0.3 g were mixed to prepare a second mixed solution.
  • the wavelength conversion layer 7 is formed by spraying the second mixed liquid on the wavelength conversion layer 7 using the coating apparatus 10 so as to have a maximum film thickness that does not cause cracks after baking, and heating and baking at 150 ° C. for 1 hour.
  • a ceramic layer 8 was produced while fixing the phosphor.
  • phenyl silicone (KER-6000; manufactured by Shin-Etsu Chemical Co., Ltd.) is applied onto the ceramic layer 8 by using a dispenser, and heated at 150 ° C. for 1 hour to cure, thereby producing the silicone sealing layer 11.
  • the light emitting device 100 was obtained.
  • a spray pressure and the moving speed of the moving stand 20 are adjusted suitably.
  • smectite (Lucentite SWN, manufactured by Corp Chemical Co., hereinafter abbreviated as SWN) which is a swellable particle, 0.05 g of RX300 which is an inorganic particle, and a solvent
  • a first mixed liquid was prepared by mixing 1.5 g of propylene glycol.
  • a wavelength conversion layer 7 was produced under the same conditions as in Example 1 using this first mixed solution.
  • 1 g of a polysiloxane dispersion and 0.3 g of a TiO 2 slurry dispersion having an average particle diameter of 20 nm were mixed to prepare a second mixture.
  • the ceramic layer 8 was produced on the same conditions as Example 1 using this 2nd liquid mixture.
  • the silicone sealing layer 11 was produced on the same conditions as Example 1 using phenyl silicone, and the light-emitting device 100 was obtained.
  • First mixing is performed by mixing 1 g of the phosphor prepared by the above preparation example, 0.05 g of synthetic mica that is a swellable particle, 0.05 g of RX300 that is an inorganic particle, and 1.5 g of propylene glycol that is a solvent.
  • a liquid was prepared.
  • a wavelength conversion layer 7 was produced under the same conditions as in Example 1 using this first mixed solution.
  • the ceramic layer 8 was produced on the same conditions as Example 1 using this 2nd liquid mixture.
  • the silicone sealing layer 11 was produced using phenyl silicone under the same conditions as in Example 1, and the light emitting device 100 was obtained.
  • First mixing is performed by mixing 1 g of the phosphor prepared by the above preparation example, 0.05 g of synthetic mica that is a swellable particle, 0.05 g of RX300 that is an inorganic particle, and 1.5 g of propylene glycol that is a solvent. A liquid was prepared. Using this first mixed solution, a wavelength conversion layer was produced under the same conditions as in Example 1. Next, 1 g of a polysiloxane dispersion and 0.3 g of isopropyl alcohol were mixed to prepare a second mixed solution. Using this second mixed solution, a ceramic layer 8 was produced under the same conditions as in Example 1, and a light emitting device 100 was obtained. (Evaluation, examination)
  • FIG. 5 shows the result.
  • the luminous efficiency was evaluated by measuring the total luminous flux of the light emitting device with a spectral radiance meter (CS-2000, manufactured by Konica Minolta Sensing) and making a relative comparison using the total luminous flux of Comparative Example 1 as a reference.
  • CS-2000 spectral radiance meter
  • the evaluation of the resistance to sulfuration was performed by measuring the total luminous flux of the light emitting device before and after the degradation test, and comparing the total luminous flux of each light emitting device after the degradation test relative to the total luminous flux of each light emitting device before the degradation test.
  • the deterioration test was performed by putting the light emitting device and sulfur powder in a sealed container and leaving them at 80 ° C. for one day.
  • the evaluation of chromaticity is a comparison and evaluation of chromaticity uniformity.
  • the chromaticity of light emission of each light-emitting device is measured using a spectral radiance meter (CS-1000A, manufactured by Konica Minolta Sensing). Evaluation was performed as follows. Five samples of each example and comparative example were prepared, and the chromaticity was measured for each sample, and the standard deviation of chromaticity was determined. The average chromaticity standard deviation is greater than 0.01 and less than or equal to 0.02 with no practical chromaticity variation (can be used sufficiently in applications where color uniformity is required, such as lighting. "O” as the degree), and "X” as a value larger than 0.02 as impractical.
  • Comparative Example 1 does not have the wavelength conversion layer 7 and the ceramic layer 8 referred to in the above embodiment, and a silicone sealing layer containing a phosphor is provided. As a result, the phosphor has settled and the chromaticity varies greatly. Moreover, it cannot be said that the light extraction efficiency (light emission efficiency) is very good, and the sulfuration resistance is low.
  • Comparative Example 2 has the wavelength conversion layer 7 and the ceramic layer 8 referred to in the above embodiment, the phosphors are uniformly dispersed, and the variation in chromaticity is within a practically acceptable range.
  • the silicone sealing layer 11 is not provided, the sulfurization resistance is low, and the luminous efficiency is worse than that of Comparative Example 1 having the silicone sealing layer.
  • Examples 1 to 6 have the wavelength conversion layer 7 and the ceramic layer 8, the phosphors are uniformly dispersed, and variations in chromaticity are in a range where there is no practical problem. Furthermore, since it has the silicone sealing layer 11, it has high sulfidation resistance and good luminous efficiency. Examples 1 to 6 show that the present invention can be carried out using various swellable particles, inorganic particles, and a translucent ceramic material.
  • the wavelength conversion unit 6 reduces the occurrence of color unevenness to an extent that it can be sufficiently used in applications where color uniformity is required, such as illumination, and has anti-sulfurization performance and light.
  • the extraction efficiency can be improved.
  • LED board 3 LED element (light emitting element) 5 Glass substrate (translucent substrate) 6 Wavelength Conversion Unit 7 Wavelength Conversion Layer 8 Ceramic Layer 9 Wavelength Conversion Element 11 Silicone Sealing Layer 40 First Mixed Liquid 100, 101, 102 Light-Emitting Device

Abstract

La présente invention a trait à un dispositif électroluminescent destiné à l'éclairage ou à d'autres applications où l'uniformité de couleur est recherchée. Afin de réduire l'incidence de la variation de couleur à un degré suffisamment utilisable et d'améliorer la prévention contre la sulfuration ainsi que le rendement d'extraction de lumière, le dispositif électroluminescent est fabriqué à l'aide d'un procédé comprenant : une étape consistant à appliquer sur élément électroluminescent une substance fluorescente, des particules capables de gonfler, des particules inorganiques et un premier mélange contenant un premier solvant; une étape suivante consistant à appliquer et à chauffer une céramique translucide et un second mélange contenant un second solvant; et une étape suivante consistant à appliquer et à chauffer un matériau d'étanchéité en silicone.
PCT/JP2013/052433 2012-02-13 2013-02-04 Élément de conversion de longueur d'onde et son procédé de fabrication et dispositif électroluminescent et son procédé de fabrication WO2013121903A1 (fr)

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US14/377,649 US20160013368A1 (en) 2012-02-13 2013-02-04 Wavelength conversion element and method for manufacturing same, and light-emitting device and method for manufacturing same

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JP6966851B2 (ja) * 2016-03-18 2021-11-17 日東電工株式会社 光学部材、ならびに、該光学部材を用いたバックライトユニットおよび液晶表示装置
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US11239213B2 (en) 2019-05-17 2022-02-01 Applied Materials, Inc. In-situ curing of color conversion layer in recess
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